Method of and apparatus for producing hydrocarbons



W. MNDR. .METHOD 0F AND APPARATUS FOR P RODUCING HYDROCARBONS.

APPLICATION FILED DECl 3 1. |915.

Patented Oct. 1D, 1922.,

WLHELBII MNDER, 0F ESLXNGJEN, GERMANY, ASSIGNGR, BY MESNE ASSIGNMENTS,

TO THE CHEMICAL FOUNDATION, NC.,

A CORPQRATXN Oli' DELAWARE.

METHOD 0F AND APPARATUS FOR ERODUCING: HYDROCARBGNS.

Application :filed December 31, 1915.

To alt whom t may concern.'

Be it .known that 1WILHELM MNDER, chemist residing at Eislingen, in the Kingdom of lurttembergfGermany, has in vented a certain new and useful improved Method of and Apparatus for Producing Hydrocarbons, of which the following is a specification.

My invention relates to an improved method of and apparatus for producing light hydrocarbons free from sulphur, as-l phalt and water from heavy mineral oiis and their residual products, such as petroleum-pitch, saponifiable oil and the like, which latter products may contain a large amount of sulphur, asphalt and water and no components boiling below a temperature of 300 C.

According -to the present invention my improved method is performed by using two distilling processes at diii'erent pressures.

ln opposition to the prior processes it is possible with my novel method to obtain in a continuous cycle of operations pure hydrocarbons boiling at a temperature between 40 and 280O C. even with such residues which contain up to 50% of water, without a previous freeing or depriving of said residues from water bemg necessary, whilst this is quite unavoidable in the methods known up to present. The hydrocarbons obtained with my improved process are free from sulphur and asphalt, 'even on using residues contain ing a high percentage of sulphur and asphalt.

The process forming the object of the prescnt invention is carried out in such a way that iirst the raw or crude materials to be treated aresubjected to distillation process under the influence of a small eXcess of pressure above the' atmospheric pressure. It appears that by employing a small overpressure a product free from asphalt and water can be obtained, said product being almost free oi' sulphur, because, the sulphur compounds are decomposed and escape in form of sulphuretted hydrogen, whilst all substances containing asphalt remain in the reacting vessel Ain the form of coke. y l

The product resulting from said first treatment, which sometimes contains small quantities of sulphur, is, at thefsame rate as it enters into the apparatus, drawn 0H from said apparatus by a pump and led into a horizontal autoclave, so that the process is,

high pressure o1 say 15 amounts to about 90% Serial No. 69,590.

continuous, with respect to the gaseous products, from the very starting of the treatment o 'f'the raw or crude material up to the obtaining -of the Iinal product. ln the autoclave the resulting product, in order to -further split up the light hydrocarbons already obtained into quite light hydrocarbons and to remove the last sulphur compounds, is preferably heated so as to aford a relatively atmospheres, and subsequently, by automatic opening of-the valve adjusted to a corresponding pressure, i. e. l5 atmospheres, said product is slowly and uninterruptedly distilled at the same pressure. The temperature is preferably maintained between 300 and 400 C. The last sulphur compounds are decomposed and are drawn ofi1 in the form of sulphuretted hydrogen. The yield of light hydrocarbons free from sulphur, asphalt and water of the original product. The greater part of these hydrocarbons boils at a temperature of 40o-200 C., the boiling temperature of the other hydrocarbons being 20G-280o C.

Thel working in both steps of the process, i. e. the distillation at a low pressure, as well as the distillation carried out at a comparatively high pressure, is continuous providing two stills for the preliminary treatment are employed so that when it becomes necessary to remove the coke from the one the other may carry on the operation. p

In the accompanying drawing forming a part of this specification an apparatus for carrying o-ut the process forming the object of my invention is represented.

The raw or crude material Hows from a container l through a pipe 2 provided with a check-valve or an obturator 3 into the distilling vessel 4 heated to about 300 C. The container 1 is arranged about 6 meters above the vessel. The raw material flowing into the vessel is vaporized and the vapors as well as the aqueous vapour which may have been generated from the water contained in the raw material are led by a pipe 5 into a cooler or condenser 6 in which they are condensed. This operation may be accelerated by slightly exhausting-the vapours in question. The very iuid condensed product gathered in a receiver 7 is at once separated from the water and can be segregated or decanted from said water by means of a siphon 18 and the like. Even when the raw or crude material contains 5-8% of lsulphur the distilled product is nearly free from sulphur, Whilst the Whole asphalt soluble in benzin, ether and alcohol remains in the distilling or cracking vessel 4 in form of coke. By using distilling vessels 'which are alternately operated and cleaned, the method becomes quite continuous.

The products of distillation free from water and asphalt which still contain traces of sulphur, in order to remove the remaining sulphur and for the sake of further decomposition or splitting up into quite light hydrocarbons, are led by means of a pump 8 through a pipe 9 provided With a non-return valve 10 into a horizontal autoclave 11 having an outlet-pipe 14, and in said autoclave 11 said products of distillation are brought to an overpressure of about 15 atmospheres by being heated to A300C-4:00". As soon as this pressure is reached, the vapours are conducted into a cooler or condenser 16 and are condensed therein. The condensed product is then gathered in a'receiver 17.

Also this step of my improved method or process is rendered continuous by inserting the non-return valve 10 into the filling-tube 9 in the path from the vessel 7 to the autoclave 11, because a segregation of coke in the autoclave no longer takes place in consequence of the preliminary -treatment referred to.

rIhe obtained condensed products are free from Water, sulphur and asphalt and, as a rule, have a boiling temperature of 40o-2000. Further, said products of condensation are free from the Well known odour or smell: Moreover, said products even after being kept for a number of years show no subsequent darkening ater refining.

Having thus vdescribed my invention,-What.

I claim and desire to secure by Letters Pat- A ent of the United States is iastate water, Which comprises subjecting heavy hydrocarbons and their residual products to a first distillation at about atmospheric pressure, condensing the vapor, and then heating, With continuous distillation, in an autoclave under a pressure above atmospheric.

2. The process for the production of light hydrocarbons free from sulphur, asphalt and Water, which comprises distillingl heavy hydrocarbons and their residual products at a temperature of about 300o C. and at a pressure of about one atmosphere, condensing the vapor, and then heating., With continuous distillation, in an autoclave under a pressure above atmospheric.

3. The process for the production of light hydrocarbons free from sulphur, asphalt and Water, which comprises distilling heavy hydrocarbons and their residual products at a temperature of about 300 C.A and at a pressure of about one atmosphere, condensing the vapor, and at once continuously distilling in an autoclave at a temperature of about 300 C. to about 400 C. and at a pressure of about 15 atmospheres, and finally condensing the vapors.

4. An apparatus for obtaininglight hydrocarbons free from sulphur, asphalt and Water, consistingof a distilling vessel, a container raised above and connected with the distilling vessel by a valve pipe, a condenser connected With said distilling vessel, a re`- ceiver connected With the condenser and adapted With a siphon for the removal of the condensed Water, an autoclave with a valve pipe connecting said autoclave with said receiver, a pump 1n said pipe, 'and a condenser connected vvith said autoclave.

In testimony whereof I aiiixed my' signature in presence of tWo Witnesses.

WILHELM MNDER. 

